Three hybrid inorganic/organic adsorbents based on alumina and phenylazoformic acid 2-phenylhydrazide were synthesized, characterized and examined for their heavy metal sorption properties. The main purpose of this research paper is to study and explore the combined hybrid characters of inorganic/organic sorbents for the selective removal and preconcentration of heavy metals via static and dynamic solid phase techniques from industrial wastewater and drinking tap water samples as well. The hybrid inorganic/organic adsorbents were identified as strongly resistive to leaching in solutions with pH 1-7 and thermally stable up to 350 degrees C. Optimization of heavy metal removal by implementation of newly designed hybrid inorganic/organic adsorbents was studied in presence of various factors as the effect of pH of contact solution and reaction time via determination of the metal sorption capacity and distribution coefficient. The hybrid adsorbents were successfully implemented for the selective removal of Pb(II), Cu(II), Fe(III), and Cr(III) from industrial wastewater samples with recovery values in the range of 91-99 +/- 2-3% as well as 98-99 +/-1-3% for the selective preconcentration of Pb(II), Cu(II), and Cr(III) from drinking tap water samples without noticeable interference caused by the matrix effect.